CN108704657B - Red phosphorus/graphite phase carbon nitride composite nanosheet and preparation method and application thereof - Google Patents

Red phosphorus/graphite phase carbon nitride composite nanosheet and preparation method and application thereof Download PDF

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CN108704657B
CN108704657B CN201810551915.XA CN201810551915A CN108704657B CN 108704657 B CN108704657 B CN 108704657B CN 201810551915 A CN201810551915 A CN 201810551915A CN 108704657 B CN108704657 B CN 108704657B
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nitride composite
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王万军
安太成
李桂英
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Guangdong University of Technology
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Abstract

The invention provides a red phosphorus/graphite phase carbon nitride composite nanosheet and a preparation method and application thereof. The red phosphorus/graphite phase carbon nitride composite nanosheet is prepared from elemental red phosphorus and bulk carbon nitride as raw materials by a one-step ultrasonic synthesis method. And stripping the bulk-phase carbon nitride into carbon nitride nanosheets under the auxiliary action of red phosphorus in the ultrasonic process, and simultaneously crushing the red phosphorus into nano red phosphorus in the ultrasonic process and loading the nano red phosphorus on the carbon nitride nanosheets to form the red phosphorus/graphite-phase carbon nitride composite nanosheets. The composite nanosheet can be used as a photocatalyst to realize the application of photocatalytic sterilization under wide-spectrum visible light, and has the capability of photocatalytic hydrogen production. The red phosphorus load greatly expands the visible light response range of the catalyst, improves the photocatalytic sterilization efficiency, does not contain any metal component, has the characteristics of simple preparation method and low cost, and has potential application value in the fields of environmental protection and clean energy production.

Description

Red phosphorus/graphite phase carbon nitride composite nanosheet and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a preparation method and application of a non-metal composite nanosheet catalyst based on red phosphorus and graphite-phase carbon nitride.
Background
The graphite phase carbon nitride has a unique layered structure and excellent chemical stability, and is applied to the fields of photocatalytic sterilization and hydrogen production as a non-metallic photocatalyst in recent years. However, the visible light response range is low (the response wavelength is below 440 nm), which severely restricts the utilization of the whole solar spectrum, so that the further improvement of the visible light utilization range and the quantum efficiency are problems to be solved. Meanwhile, the elemental red phosphorus is discovered in recent years to be an excellent photocatalytic material, the response light range of the elemental red phosphorus reaches about 700nm, most visible light spectrums are covered, the elemental red phosphorus is the earliest discovered elemental photocatalytic sterilization catalyst, and meanwhile, the elemental red phosphorus has the photocatalytic hydrogen production capability. However, the smaller band gap of the material results in higher rate of photo-generated electron-hole recombination, which is not favorable for the photocatalytic reaction. Therefore, the graphite phase carbon nitride with a wider band gap and the elemental red phosphorus are compounded to form the heterojunction, the problem of small photoresponse of the graphite phase carbon nitride can be solved, and meanwhile, the photo-generated electron-hole recombination rate is reduced due to the formation of the heterojunction, so that the photocatalytic quantum efficiency and the sterilization efficiency can be greatly improved.
At present, the compounding of elemental red phosphorus and carbon nitride is only limited to simple mechanical mixing of bulk materials, but the improvement of the photocatalytic performance is very limited. Research shows that the layered bulk graphite phase carbon nitride material is stripped to form a nanosheet, so that the photoproduction electron-hole separation rate can be further improved. Therefore, the development of a material preparation method is to load the simple substance red phosphorus on the graphite-phase carbon nitride nano-sheet to realize the composite catalyst with wide spectral response and high electron-hole separation rate. In this respect, the ultrasonic synthesis method can crush the monomeric red phosphorus to form nano-scale red phosphorus particles, can be used as an intercalation material to assist the liquid phase stripping of the graphite phase carbon nitride, and can lead the nano red phosphorus to be simultaneously combined and loaded on the carbon nitride nano-sheet by chemical bonds to form the red phosphorus/graphite phase carbon nitride composite nano-sheet by the local high temperature and high pressure formed by the ultrasonic cavitation effect.
Until now, no research and report about the preparation method of the red phosphorus/graphite phase carbon nitride composite nanosheet and the wide spectral response photocatalytic sterilization and hydrogen production related to the preparation method are found.
Disclosure of Invention
The invention aims to overcome the defects of a single photocatalyst in the aspects of photoresponse range and photocatalytic performance, develop a red phosphorus/graphite phase carbon nitride composite nanosheet photocatalyst, provide an economic and cheap one-step synthesis method for preparing the catalyst and greatly reduce the application cost.
The invention aims to provide a preparation method of a composite nanosheet based on red phosphorus and graphite-phase carbon nitride.
The invention also aims to provide the composite nanosheet based on red phosphorus and graphite-phase carbon nitride, which is prepared by the method.
It is a further object of the present invention to provide the use of the above-mentioned composite nanoplatelets based on red phosphorus and graphite-phase carbon nitride.
The above purpose of the invention is realized by the following technical scheme:
the red phosphorus/graphite phase carbon nitride composite nanosheet is prepared by combining red phosphorus and bulk graphite phase carbon nitride and adopting an ultrasonic synthesis method.
A preparation method of red phosphorus/graphite phase carbon nitride composite nanosheets comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
s2, purifying red phosphorus by a hydrothermal method;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
Preferably, the precursor in step S1 is cyanamide, dicyandiamide, melamine, urea or thiourea.
Preferably, in the thermal polymerization method in step S1, the heating is performed at a constant temperature of 480 to 620 ℃ for 1.5 to 2.5 hours at a heating rate of 2 to 10 ℃/min.
Preferably, the reaction temperature of the hydrothermal method in the step S2 is 100 to 200 ℃, and the reaction time is 2 to 12 hours.
Preferably, the mass ratio of the added purified red phosphorus and the bulk graphite phase carbon nitride in the step S3 is 0.5: 1-4: 1.
Preferably, the water adding amount in the step S3 is 20-150 mL.
Preferably, the ultrasonic frequency of the ultrasonic treatment in the step S3 is 20-50 kHz, and the ultrasonic time is 4-15 h.
The application of the red phosphorus/graphite phase carbon nitride composite nanosheet in broad-spectrum photocatalytic sterilization is characterized in that the photoresponse wavelength range of the broad-spectrum photocatalysis is 420-700 nm.
The application of the red phosphorus/graphite phase carbon nitride composite nanosheet in hydrogen production by broad-spectrum photocatalysis is characterized in that the photoresponse wavelength range of the broad-spectrum photocatalysis is 420-700 nm.
Compared with the prior art, the invention has the beneficial effects that: the invention combines the single red phosphorus and the graphite phase carbon nitride, and prepares the red phosphorus/graphite phase carbon nitride composite nanosheet in one step by adopting an ultrasonic synthesis method, thereby greatly reducing the preparation cost. The red phosphorus/graphite phase carbon nitride composite nanosheet photocatalyst prepared by the invention can realize the application of wide-spectrum response photocatalytic sterilization and photocatalytic hydrogen production, and the sterilization and hydrogen production efficiency is higher than that of pure red phosphorus and carbon nitride.
Drawings
FIG. 1 is a transmission electron micrograph of a red phosphorus/graphite phase carbon nitride composite nanoplatelet material according to the present invention;
fig. 2 is a graph comparing the photocatalytic sterilization efficiency of the red phosphorus/graphite phase carbon nitride composite nanosheets of the present invention with pure red phosphorus and carbon nitride.
FIG. 3 is a graph showing the photocatalytic hydrogen production efficiency at different wavelengths of the red phosphorus/graphite phase carbon nitride composite nanosheet material of the present invention.
Detailed Description
The invention is further described in the following description with reference to the figures and specific examples, which should not be construed as limiting the invention. It is within the scope of the present invention to make simple modifications or alterations to the methods, procedures or conditions of the present invention without departing from the spirit and substance of the invention; unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1:
this example is a specific example of preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets.
The red phosphorus/graphite phase carbon nitride composite nanosheet is prepared by combining red phosphorus and bulk graphite phase carbon nitride and adopting an ultrasonic synthesis method.
The preparation method of the red phosphorus/graphite phase carbon nitride composite nanosheet comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
the method specifically comprises the following steps: selecting melamine as a precursor, placing 5g of melamine in a crucible, heating at 550 ℃ for 2 hours at a constant temperature (the heating rate is 5 ℃/min), after the temperature is cooled, grinding a sample into yellow powder to obtain a graphite-phase carbon nitride phase material, and storing the graphite-phase carbon nitride phase material in a dryer for later use;
s2, purifying red phosphorus by a hydrothermal method;
2g of commercial elemental red phosphorus was added to a 20mL polytetrafluoroethylene-lined reaction vessel, 15mL of water was added, and the reaction vessel was placed in an oven and heated at a constant temperature of 200 ℃ for 10 hours. Centrifuging, washing and drying the solid product to obtain red powdered purified red phosphorus, and storing the red powdered purified red phosphorus in a dryer for later use;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
And (3) placing 0.1g of bulk graphite phase carbon nitride obtained in the step and 0.15g of purified red phosphorus obtained in the step into a glass container, adding 40mL of deionized water, mixing, stirring for 10min, and then placing into an ultrasonic instrument for ultrasonic treatment with the frequency of 35kHz and the ultrasonic time of 6 h. And after the reaction is finished, centrifuging, washing and drying the obtained turbid liquid to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
Example 2:
this example is a specific example of preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets.
The red phosphorus/graphite phase carbon nitride composite nanosheet is prepared by combining red phosphorus and bulk graphite phase carbon nitride and adopting an ultrasonic synthesis method.
The preparation method of the red phosphorus/graphite phase carbon nitride composite nanosheet comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
the method specifically comprises the following steps: selecting melamine as a precursor, placing 5g of melamine in a crucible, heating at 480 ℃ for 1.5 hours (the heating rate is 2 ℃/min), after the temperature is cooled, grinding a sample into yellow powder to obtain a graphite-phase carbon nitride phase material, and storing the graphite-phase carbon nitride phase material in a dryer for later use;
s2, purifying red phosphorus by a hydrothermal method;
2g of commercial elemental red phosphorus was added to a 20mL polytetrafluoroethylene-lined reaction vessel, 15mL of water was added, and the reaction vessel was placed in an oven and heated at 100 ℃ for 2 hours. Centrifuging, washing and drying the solid product to obtain red powdered purified red phosphorus, and storing the red powdered purified red phosphorus in a dryer for later use;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
And (3) placing 0.1g of bulk graphite phase carbon nitride obtained in the step and 0.05g of purified red phosphorus obtained in the step into a glass container, adding 20mL of deionized water, mixing, stirring for 10min, and then placing into an ultrasonic instrument for ultrasonic treatment with the frequency of 20kHz and the ultrasonic time of 4 h. And after the reaction is finished, centrifuging, washing and drying the obtained turbid liquid to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
Example 3:
this example is a specific example of preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets.
The red phosphorus/graphite phase carbon nitride composite nanosheet is prepared by combining red phosphorus and bulk graphite phase carbon nitride and adopting an ultrasonic synthesis method.
The preparation method of the red phosphorus/graphite phase carbon nitride composite nanosheet comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
the method specifically comprises the following steps: selecting melamine as a precursor, placing 5g of melamine in a crucible, heating at the constant temperature of 620 ℃ for 2.5 hours (the heating rate is 10 ℃/min), after the temperature is cooled, grinding a sample into yellow powder to obtain a graphite phase carbon nitride phase material, and storing the graphite phase carbon nitride phase material in a dryer for later use;
s2, purifying red phosphorus by a hydrothermal method;
2g of commercial elemental red phosphorus was added to a 20mL polytetrafluoroethylene-lined reaction vessel, 15mL of water was added, and the reaction vessel was placed in an oven and heated at a constant temperature of 200 ℃ for 12 hours. Centrifuging, washing and drying the solid product to obtain red powdered purified red phosphorus, and storing the red powdered purified red phosphorus in a dryer for later use;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
And (3) placing 0.1g of bulk graphite phase carbon nitride obtained in the step and 0.4g of purified red phosphorus obtained in the step into a glass container, adding 150mL of deionized water, mixing, stirring for 10min, and then placing into an ultrasonic instrument for ultrasonic treatment with the frequency of 50kHz and the ultrasonic time of 15 h. And after the reaction is finished, centrifuging, washing and drying the obtained turbid liquid to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
Example 4:
this example is a specific example for measuring the photocatalytic bactericidal performance of the prepared red phosphorus/graphite phase carbon nitride composite nanosheet.
The photocatalytic sterilization performance test is carried out in a quartz glass reactor. Coli (e.coli) was selected as the target inactivated bacteria. Culturing Escherichia coli at 37 deg.C for 16 hr to obtain stationary phase strain, centrifuging, collecting, diluting with 0.9% NaCl solution to 1 × 107cfu/mL of bacterial solution. Adding 50mg of red phosphorus/graphite phase carbon nitride composite nanosheet catalyst into 50mL of the bacterial solution, placing the bacterial solution in a dark place, stirring the bacterial solution for 10min, then turning on a xenon lamp light source (provided with band-pass visible light filters (lambda is 420,500,550,600,650,700nm) with different wavelengths to start reaction, and calculating the number of bacterial colonies by using a flat plate counting method, as shown in fig. 2, the prepared red phosphorus/graphite phase carbon nitride composite nanosheet can completely kill 1 × 10 within 80min7The effect of cfu/mL bacteria is obviously higher than that of pure red phosphorus and graphite phase carbon nitride. Experimental results show that the red phosphorus/graphite phase carbon nitride composite nanosheet photocatalyst prepared by the invention is a novel photocatalytic sterilization material with wide spectral response and high activity.
Example 5:
this example is a specific example for measuring the photocatalytic hydrogen production performance of the prepared red phosphorus/graphite phase carbon nitride composite nanosheet.
The photocatalytic hydrogen production performance test is carried out in a closed quartz reactor. 40mg of red phosphorus/graphite phase carbon nitride composite nanosheet catalyst was dispersed in 45mL of deionized water, and 5mL of triethanolamine was added as a sacrificial agent. The reaction vessel is vacuumized, placed in a dark place and stirred for 10min, then a xenon lamp light source (equipped with band-pass visible light filters (lambda is 420,500,550,600,650,700nm) with different wavelengths) is turned on to start reaction, and the yield of hydrogen is detected by utilizing gas chromatography, as shown in figure 3, the prepared red phosphorus/graphite phase carbon nitride composite nanosheet can realize photocatalytic hydrogen production under different wavelengths of a broad spectrum, and the longest wavelength of the prepared red phosphorus/graphite phase carbon nitride composite nanosheet can be extended to 700 nm.
The above-described embodiments of the present invention are merely preferred embodiments of the present invention, and are not intended to limit the embodiments of the present invention. Other variations will be apparent to persons skilled in the art upon consideration of the foregoing description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. A red phosphorus/graphite phase carbon nitride composite nanosheet is characterized in that: the red phosphorus/graphite phase carbon nitride composite nanosheet is prepared by combining red phosphorus and bulk graphite phase carbon nitride and adopting an ultrasonic synthesis method;
the method comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
s2, purifying red phosphorus by a hydrothermal method;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
2. The method for preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets according to claim 1, wherein: the method comprises the following steps:
s1, selecting a proper precursor, and preparing a bulk graphite phase carbon nitride material by adopting a thermal polymerization method;
s2, purifying red phosphorus by a hydrothermal method;
and S3, adding water to the bulk graphite phase carbon nitride and the purified red phosphorus, mixing, performing ultrasonic treatment, centrifuging, washing and drying the obtained suspension to obtain the red phosphorus/graphite phase carbon nitride composite nanosheet.
3. The method for preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets of claim 2 wherein the precursor of step S1 is cyanamide, dicyandiamide, melamine, urea or thiourea.
4. The method for preparing red phosphorus/graphite phase carbon nitride composite nanosheets according to claim 2, wherein the thermal polymerization method in step S1 is heating at a constant temperature of 480-620 ℃ for 1.5-2.5 hours at a rate of temperature rise of 2-10 ℃/min.
5. The method for preparing red phosphorus/graphite phase carbon nitride composite nanosheets according to claim 2, wherein the hydrothermal method of step S2 has a reaction temperature of 100-200 ℃ and a reaction time of 2-12 hours.
6. A method for preparing red phosphorus/graphite phase carbon nitride composite nanoplatelets according to claim 2, wherein the mass ratio of the added purified red phosphorus to the bulk graphite phase carbon nitride in step S3 is 0.5: 1-4: 1.
7. The method for preparing red phosphorus/graphite phase carbon nitride composite nanosheets according to claim 2, wherein the amount of water added in step S3 is 20-150 mL.
8. The preparation method of the red phosphorus/graphite phase carbon nitride composite nanosheet according to claim 2, wherein the ultrasonic frequency of the ultrasonic treatment in step S3 is 20-50 kHz, and the ultrasonic time is 4-15 h.
9. The application of the red phosphorus/graphite phase carbon nitride composite nanosheet of claim 1 in broad-spectrum photocatalytic sterilization, wherein the photoresponse wavelength range of the broad-spectrum photocatalysis is 420-700 nm.
10. The application of the red phosphorus/graphite phase carbon nitride composite nanosheet in hydrogen production through broad-spectrum photocatalysis, which is disclosed by claim 1, wherein the photoresponse wavelength range of the broad-spectrum photocatalysis is 420-700 nm.
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